Determination of trace iron in high-purity quartz by cool flame mode-inductively coupled plasma mass spectrometry
ZHANG Hongli1,2,3, NI Wenshan1,2,3, LIU Lei1,2,3, XIAO Fang1,2,3
1. Zhengzhou Institute of Multipurpose Utilization of Mineral Resources, CAGS, Zhengzhou 450006, China; 2. China National Engineering Research Center for Utilization of Industrial Minerals, Zhengzhou 450006, China; 3. Northwest China Center for Geoscience Innovation, Xi’an 710054, China
Abstract：Iron is an important indicator element for the grading of quartz sand products, so it is very important to determine its content rapidly and accurately. During the determination of iron by inductively coupled plasma mass spectrometry (ICP-MS), it will be interfered by the polyatomic molecular ion of ArO+.The high-purity quartz sample was dissolved with hydrofluoric acid and nitric acid. The testing element was extracted with nitric acid and determined in cool flame mode, eliminating the interference of polyatomic molecular ion (ArO+). 100 ng/mL cobalt was used as internal standard element and 56Fe was the isotope. The determination method of trace iron in high-purity quartz sample by ICP-MS was established. The radio-frequency power, sampling depth and matrix mass concentration were optimized. The radio-frequency power of 850 W and sampling depth of 5.3 mm were used in experiments. The mass concentration of matrix was also investigated. The results showed that the matrix effect could be effectively overcome by controlling the sample amount and diluting the sample solution (the mass concentration of matrix in testing solution should be not higher than 10 mg/mL). Under the optimized experimental conditions, the mass concentration of iron in range of 0.100-100 ng/mL was linearly correlated to the mass spectrometry intensity. The correlation coefficient was 0.999 6. When the sample amount was 1.000 0 g, the limit of detection was 0.039 μg/g, and the limit of quantification was 0.13 μg/g. The contents of iron in five high-purity quartz samples with different iron content levels were determined according to the experimental method (n=9). Moreover, the standard addition test and method comparison test were also conducted. The found results were basically consistent with those obtained by ICP-MS in kinetic energy discrimination collision cell mode. The relative standard deviations (RSD) were between 3.2% and 5.1%, and the recoveries were between 96% and 102%.
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